顶空/气相色谱-串联质谱法测定合成洗涤剂及化妆品中二噁烷残留

Determination of 1,4-Dioxane Residues in Synthetic Detergents and Cosmetics by Headspace/Gas Chromatography-Tandem Mass Spectrometry

建立了顶空/气相色谱-串联质谱(HS/GC-MS/MS)测定合成洗涤剂和化妆品中二噁烷含量的分析方法。将样品与适量的水混溶,加入固体氯化钠产生"盐析"效应后再通过超声振荡,使样品中的二噁烷充分溶解。此后将样品瓶于80℃混合摇振30 min达到气液平衡,顶空进样,在GC-MS/MS多反应监测模式(MRM)下测定,二噁烷在质量浓度0.1～100 mg/L范围内呈良好线性,相关系数为0.999 8,检出限(S/N=3)为0.010 mg/kg,定量下限(S/N=10)为0.035 mg/kg,平均加标回收率为98%～103%,相对标准偏差为0.44%～2.1%。该方法能有效消除复杂基质的干扰,结果准确可靠,灵敏度高,重现性好,适用于合成洗涤剂和化妆品中痕量二噁烷的测定。

A headspace/gas chromatography- tandem mass spectrometric （HS/GC -MS/MS） method was established for the determination of 1, 4-dioxane residues in synthetic detergents and cosmetics. The samples were mixed with water, then sodium chloride was added to produce the ＂saltingout＂ effect. After oscillation, 1, 4-dioxane in sample was dissolved completely. The sample mixed with water was oscillated for 30 min at 80 ℃ to get gas - liquid balance state and then the upper clear gas was prepared. The detection was carried out by GC - MS/MS under the multiple-reaction monitoring （MRM） mode. Good linearity in the concentration range of 0. 1 - 100 mg/L was obtained, with a correlation coefficient of 0. 999 8. The limit of detection（LOD） was O. 010 mg/kg and the limit of quantitation（LOQ） was 0. 035 mg/kg. The average recoveries were in the range of 98% - 103% , with relative standard deviations （RSDs） of 0. 44% - 2. 1%. The accuracy, reliability and sensitivity of the method made it suitable for the determination of 1, 4-dioxane in synthetic detergents and cos metics.